反应详情

温度

-20 °C

3.03 ml of n-butyllithium (1.6M in hexane) are added dropwise at −40° C. to the suspension of 0.884 g of 3,6-diethoxy-2,5-dihydropyrazine in 12 ml of tetrahydrofuran. After 20 minutes, a solution of 1.265 g of 7-(2-bromomethyl-3-methylbutyl)-1-(2-methoxyethoxy)naphthalene in 5 ml of tetrahydrofuran is added dropwise. The reaction mixture is stirred further at −40″C. for 30 minutes, then warmed to −20° C. over 1 hour. After 18 hours, the reaction mixture is concentrated by evaporation—the residue is partitioned between ethyl acetate and water. The aqueous phase is extracted with ethyl acetate (2×)—the combined organic phases are washed successively with water (2×) and brine, dried over sodium sulphate and concentrated by evaporation. The crude title compound is identified on the basis of the Rf value from the residue.

1. waitfor 30 minutes
2. waitAfter 18 hours
3. concentrationthe reaction mixture is concentrated by evaporation—the residue
4. customis partitioned between ethyl acetate and water
5. extractionThe aqueous phase is extracted with ethyl acetate (2×)—the combined organic phases
6. washare washed successively with water (2×) and brine
7. dry with materialdried over sodium sulphate
8. concentrationconcentrated by evaporation